Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry has been demonstrated for the analysis of Taxus brevifolia extracts. The detection limit for the taxanes contained therein is estimated at 1 pmol using the matrix 4-nitroaniline at a matrix-to-analyte molar ratio of 100:1. Acquisition and calibration of the mass spectral data requires less than 5 min. The [M+H]+, [M+Na]+, and [M+K]+ ions provide mol wt confirmation and structurally significant fragment ions indicative of the various substituent groups located on the diterpene skeleton are formed.